Co、Ni及其合金纳米线阵列的制备及磁性研究

采用交流电化学沉积法,在多孔阳极氧化铝(AAO）模板孔洞中成功组装了铁磁性金属Co、Ni、CoNi合金纳米线阵列并采用扫描电子显微镜(SEM）、X射线衍射(XRD）等对样品进行表征。结果表明,Co、Ni及CoNi合金阵列体系中纳米线均匀有序,形状各向异性较大(长径比达30以上）,有显著的结晶择优取向。对Co、Ni、CoNi合金纳米线阵列体系进行磁性分析,振动样品磁强计(VSM）测试结果显示,纳米线有明显的磁各向异性,适合用作垂直磁记录介质。纳米线阵列退火后沿纳米线方向矫顽力和矩形比减小,样品的垂直磁各向异     

钴纳米线的模板制备与磁性

利用二次阳极氧化法制备了多孔阳极氧化铝模板. 用直流电化学沉积方法成功地在模板孔道内制备了钴纳米线. 采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)和振动样品磁强计(VSM)对样品的形貌、晶体结构和磁性进行了研究. 结果表明， 模板的孔径均匀, 孔道平直. 钴纳米线为多晶的六方密堆积结构. 钴纳米线具有明显的磁各向异性, 这主要起源于纳米线的形状各向异性.     

双槽法电沉积Cu/Ni多层纳米线有序阵列

以多孔阳极氧化铝（AAO）为模板，采用双槽法电沉积工艺制得高度有序的Cu/Ni多层纳米线阵列。利用扫描电镜（SEM）和透射电镜（TEM）对Cu/Ni多层纳米线进行了表征，观察到纳米线表面平滑，多层结构清晰，各子层厚度均匀，直径约为 100 nm，与AAO模板孔径基本一致。由选区电子衍射（SAED）照片可知，多层纳米线中Cu层和Ni层均为单晶结构。振动样品磁强计（VSM）测试结果表明，Cu/Ni多层纳米线阵列具有明显的垂直磁各向异性，外加磁场垂直和平行于AAO模板表面时，磁滞回线的矩形比分别为 0.701 和 0.101 ，矫顽力分别为 589 Oe和 202 Oe。通过控制铝阳极氧化工艺及电沉积时间，可获得不同直径、不同子层厚度的Cu/Ni多层纳米线阵列。     

热处理对[NiFe/Cu/Co/Cu]_n多层纳米线磁性能的影响

采用双槽控电位法在阳极氧化铝(AAO)模板中制备了有序均一的[NiFe/Cu/Co/Cu]n多层纳米线阵列,并在不同温度下进行了热处理.利用X射线衍射(XRD)对热处理前后多层线的晶体结构进行了测试.考察了不同退火温度对多层线矫顽力、剩磁比、巨磁电阻(GMR)效应、磁灵敏度的影响.随热处理温度升高,多层纳米线中磁性微晶晶型取向越来越明显,晶体结构更均匀;多层纳米线的矫顽力和剩磁比先增大后减小.300°C下多层纳米线矫顽力达到最大值,GMR最大值可达59%,对应的磁电阻灵敏度(SV)为0.233%Oe-1.     

磁场诱导制备Fe-B非晶态合金纳米线及其磁学性质

通过引入外加直流电磁场, 采用KBH4还原法在室温下制备了一维Fe-B非晶态合金纳米线, 并采用X射线衍射(XRD)、电感耦合等离子原子发射光谱仪(ICP-AES)和扫描电子显微镜(SEM)等表征方法研究了产物的结构、组成和形貌. 结果表明, 在直流电磁场的作用下得到了Fe-B非晶态合金纳米线, 所得样品的直径在50-80 nm之间, 长度达到数微米. 通过振动样品磁强计(VSM)研究其磁学性质, 发现外加磁场的引入会显著影响Fe-B非晶态合金的磁学性质. 随着引入磁场强度的增强, 所得样品的饱和磁感应强度和矫顽力明显区别于未引入磁场制备的Fe-B非晶态合金.     

单晶Ni纳米线阵列的制备与磁性能

采用恒电流沉积方法, 在多孔阳极氧化铝(AAO)模板中制备出了具有单晶结构的Ni纳米线阵列. 采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线衍射(XRD)技术对制备的Ni纳米线阵列的形貌及结构进行了表征. 利用振动样品磁强计(VSM)对单晶Ni纳米线阵列的磁性能进行了研究. 结果表明, 单晶镍纳米线阵列的易磁化方向为纳米线轴向, 并且与多晶纳米线相比显示出了更高的矫顽力. 直径为30 nm的纳米线具有较高的矫顽力(8.236×104 A/m)和较高的剩磁比(Mr＝0.94Ms).     

Fe-Co-Ni合金纳米线有序阵列的模板合成与磁性

以二次阳极氧化的氧化铝膜为模板，用电化学沉积的方法成功地合成了Fe-Co-Ni三组份有序纳米线阵列.扫描电子显微镜（SEM）和透射电子显微镜(TEM)观察表明纳米线表面光滑、有序、高长径比；磁性测量表明,其矫顽力较同组份的膜材料有较大的提高.将样品在惰性气体氛围中不同温度下退火，随着退火温度增加，其纵向矫顽力有一个极值，而对应的横向矫顽力没有类似的变化，关于这一现象的机理,本文进行了初步的讨论. 图5参15     

Co/Cu多层纳米线阵列的制备与磁性能

利用双槽直流电沉积技术在阳极氧化铝(AAO)模板的纳米孔中获得调制波长为50 和200 nm 的Co/Cu多层纳米线, 多层纳米线的调制波长由电沉积时间控制. 运用扫描电子显微镜(SEM)和透射电子显微镜(TEM)表征纳米线的形貌, Co/Cu多层纳米线的长度约20 μm, 直径约80 nm; 用X射线衍射(XRD)研究多层线的结构; 用振动样品磁强计(VSM)测试纳米线阵列的磁性能; 利用可变磁场结合高灵敏度恒流装置研究巨磁电阻(GMR)特性. 结果表明, Co/Cu多层纳米线具有磁各向异性. 当磁场与纳米线平行和垂直时, 调制波长为50 nm的多层线的矫顽力分别为87500 和34200 A·m-1, 而调制波长为200 nm的多层线阵列的矫顽力分别为28600 和8000 A·m-1. 调制波长为50 nm的多层纳米线的磁电阻变化率高达-%, 而调制波长为200 nm的多层线未产生明显的GMR效应.     

镨元素对(Nd,Pr)10.5(FeCoZr)83.5B6合金显微结构和磁性能的影响

研究了稀土元素Pr对快淬(Nd1-xPrx)10.5(FeCoZr)83.5B6(x=0,0.2,0.4,0.6,0.8,1.0)合金显微组织结构和粘结磁体磁性能的影响。通过部分过快淬获得由非晶和微晶共同组成的条屑,在实验优化的退火条件下晶化处理后,制备出最佳磁性能的系列粘结磁体。随Pr含量的增加,磁体的内禀矫顽力Hci单调上升,剩磁Br单调下降,(BH)m在x=0.6～0.8处达到最大值70.6kJ·m-3。Pr元素使合金非晶态的晶化转变温度和转化能降低,合金的显微组织结构变得较粗大和较不均匀,从而使快淬粘结磁体剩磁降低,但Pr2Fe14B化合物较高的磁晶各向异性场使磁体的内禀矫顽力提高。     

α-铁纳米线阵列的磁矩分布

在多孔阳极氧化铝(AAO)模板中, 采用电化学方法制备出α-铁纳米线阵列复合膜. 用透射Mössbauer谱(MS)、内转换电子Mössbauer 谱(CEMS)和微磁学模拟对直径为60 nm的α-铁纳米线阵列进行了内部和端面磁矩分布的研究. 透射Mössbauer 谱的结果表明, α-铁纳米线阵列内部磁矩很好地平行于纳米线长轴方向, 而内转换电子 Mössbauer 谱观察表明, 位于纳米线阵列端面, 磁矩偏离纳米线的长轴方向分布, 由二、五峰的强度计算出平均偏角为24.0°. 另外, 用微磁学模拟方法对不同深度的磁矩分布做了数值统计, 结果表明, 在纳米线内部磁矩严格地平行于纳米线轴, 越趋近两端, 平均磁矩与纳米线轴的夹角越大. 磁性测量结果表明α-铁纳米线阵列宏观磁性表现出很强的磁各向异性.     

NixPb1-x nanowire arrays: effects of annealing

Ni(x)Pb(1-x) nanowire arrays were successfully fabricated by AC electrodeposition within the nanopores of ordered porous alumina films prepared by a two-step anodization. Transmission electron microscopy analyses showed that the Ni-Pb nanoarrays are polycrystalline with dimension uniformity around 20 nm in diameter and lengths up to several micrometers. X-ray diffraction results revealed that the face-centered-cubic (fcc) Ni and fcc Pb peaks are detected when the Ni component (x) is below 0.71, indicating that the Ni(x)Pb(1-x) nanoarrays do not form metastable phase alloy. Hysteresis loops determined by vibrating sample magnetometer indicated that the Ni(x)Pb(1-x) nanoarrays obtained possess obvious magnetic anisotropy, and the perpendicular coercivity was lower than that of pure Ni nanowries before and after annealing. Annealing under magnetic field was carried out to examine the effect of a magnetic field on magnetic properties using an electromagnet field up to 0.3 T.     

Structure and magnetic properties of Co nanowires electrodeposited into the pores of anodic alumina membranes

Cobalt nanowires were obtained in the process of electrodeposition into pores of an alumina membrane. Structural research (XRD, TEM) of Co revealed the face-centered cubic structure. However, the existence of the hexagonal structure cannot be excluded due to strong texture. The influences of an external magnetic field and Al₂O₃ membrane geometry on magnetic properties of obtained wires were examined. It was found that cobalt nanowires exhibit pronounced shape anisotropy in a direction parallel to the wire axis. The highest influence on the magnetic properties is ascribed to the nanowires geometry i.e., height, diameter, and distances between single wires. Application of an external magnetic field in a perpendicular direction to the sample surface during cobalt electrodeposition increases magnetic anisotropy with a privileged direction along the wire axis. Application of the magnetic field in a parallel direction to the sample surface changes the direction of magnetization.     

Structural, magnetic, and magnetoresistive properties of electrodeposited Ni5Zn21 alloy nanowires

Ni5Zn21 alloy nanowires were fabricated through template-assisted electrochemical deposition method. The morphology and microstructures of as-deposited nanowires were determined by field-emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), electron diffraction (ED), and electron probe microanalysis (EPMA). The accurate composition was measured via induced coupling plasma atomic emission spectroscopy. SEM results show that Ni5Zn21 nanowires are deposited in most of the nanopores of the template, and they are continuous and dense throughout the whole length. The XRD result demonstrates that the nanowires are mainly composed of a cubic gamma phase Ni5Zn21 alloy, but there also exists a trace of Zn-rich eta phase. HRTEM and ED reveal that the alloy nanowires are polycrystalline with the crystallite size of several tens of nanometers. EPMA of a single nanowire illustrates that there exist Ni-rich microzones in as-deposited nanowires. Subsequent magnetic measurements of the array also confirmed the existence of them. In addition, it can be further inferred that the shape of Ni-rich microzones is probably barlike or disklike, from the anisotropy of zero field cooling/field cooling (ZFC/FC) curves as well as the vortex magnetization behavior of the Ni5Zn21 nanowire array. The low-temperature magnetoresistance of the Ni5Zn21 nanowire array was also measured. Giant magnetoresistance instead of anisotropic magnetoresistance is suggested to be responsible for contributing to the magnetoresistance.     

Synthesis, morphology, and magnetic characterization of iron oxide nanowires and nanotubes

We have explored the synthesis of iron oxide particles, tubes, and fibrils within the pores of nanoporous polycarbonate and alumina membranes. The membranes contain uniformly distributed cylindrical pores with monodispersed diameters (varying between 20 and 200 nm) and thicknesses of 6 and 60 microm, respectively. By hydrolysis and polymerization of iron salts, particles of different sizes and phases were formed in the pores, building iron oxide particle nanowires. Alternatively, by the sol-gel technique, using as reagents metalloorganic compounds, fibrils and tubes of different iron oxide phases were prepared. Structural and morphological investigations performed using scanning electron microscopy and transmission electron microscopy revealed ordered iron oxide particle wires, tubes, and fibrils formed inside the membrane nanopores. Magnetic characterization was accomplished with a vibrating sample magnetometer. Below the blocking temperature (T(B)), the magnetic behavior of the nanowires was governed by dipolar interaction between nearest-neighbor nanoparticles inside the pore, whereas the energy barrier, and therefore the T(B) value, was mainly governed by dipolar interaction between magnetic moments over larger (interpore) distances. As expected, crystalline iron oxide nanotubes exhibited magnetic perpendicular anisotropy due to their magnetocrystalline and shape anisotropy.     

Effects of annealing temperature on magnetic property and structure of amorphous Co49Pt51 alloy nanowire arrays prepared by direct-current electrodeposition

Co49Pt51 nanowire arrays with an average diameter of 35 nm and lengths up to several micrometers were grown in an ordered porous anodic aluminum oxide (AAO) template using direct-current electrodeposition. The as-deposited samples were annealed at 100, 200, 300, 400, 500, 600, and 700 degrees C, respectively. The temperature dependence of the magnetic property of the Co49Pt51 nanowire arrays associated with the microstructure was analyzed by X-ray diffraction and a vibrating sample magnetometer. Magnetic measurements show that the samples both as-prepared and annealed at low temperatures have excellent perpendicular anisotropy. The perpendicular coercivity (Hc(perpendicular)) of Co49Pt51 alloy nanowire arrays increases dramatically as the annealing temperature (T(A)) rises, reaches a maximum(Hc(perpendicular) = 2770 Oe) at 400 degrees C, and then decreases sharply as T(A) rises further. This phenomenon should be attributed to the special structure of the nanowire arrays/AAO, and the microstructure factors significantly change during the annealing process.     

NiB和NiP超细非晶合金的退火晶化行为及催化性能

 采用X射线吸收精细结构（XAFS）,X射线衍射（XRD）和差热分析（DTA）等方法研究了以化学还原法制备的NiB和NiP超细非晶态合金催化剂在退火过程中的结构变化．XRD结果表明,在300℃下退火时,NiB超细非晶态合金晶化生成纳米晶Ni3B亚稳物相,NiP超细非晶态合金则主要晶化生成金属Ni和部分晶态Ni3P的混合物相;在500℃退火且近于完全晶化的条件下,大部分超细非晶态合金都晶化为金属Ni．XAFS结果定量地说明,对于NiB和NiP初始样品,第一近邻Ni－Ni配位的平均键长Rj分别为0.274和0.271nm,其结构无序度σS很大,分别为0.033和0.028nm,其热无序度σT分别为0.0069和0.0060nm．300℃退火后,晶化生成的Ni3B的Ni－Ni配位的σS降低到初始样品的33％,仅为0.011nm．500℃退火后,NiB样品的结构参数与金属Ni基本一致,但NiP样品的Ni－Ni配位的σS还远大于σT,仍为0.0125nm,表明NiB和NiP超细非晶态合金的退火晶化行为有很大的差别．纳米晶Ni3B催化苯加氢反应的转化率比超细Ni－B非晶态合金或多晶金属Ni更高,表明纳米晶Ni3B中的Ni与B原子组成了苯加氢催化反应的活性中心．     

低温熔盐中电沉积Sm-Co合金膜及其磁性能

在353 K的尿素-乙酰胺-NaBr-KBr熔体中, 用恒电位电解法在Cu基片上制备了Sm-Co合金膜. 利用循环伏安法研究了熔体的电化学行为. 电化学实验结果表明, 在Pt电极上, Co(II)+2e→Co(0)是一步完全的不可逆反应; 测得CoCl2-尿素-乙酰胺-NaBr-KBr熔体中, Co(II)在Pt电极上的传递系数α=0.31, 扩散系数D0=4.78×10^-5 cm2·s-1; Sm(III)难以单独沉积, 但能被Co(II)诱导共沉积, 在不同阴极电位下制备出不同Sm含量的非晶合金膜. 用等离子发射光谱仪(ICP)检测薄膜成分, 用SEM观察了薄膜的表面形貌结构, 用XRD和振动样品磁强计(VSM)分析样品退火前后的晶相和磁性能变化特征. 结果表明, 在923 K进行退火30 s后Sm-Co薄膜由非晶转变为多晶结构, 并以hcp晶相结构为主; 退火和Sm含量对Sm-Co合金膜的磁性能有重要的影响.     

Propriétés magnétiques des multicouches Tb/Fe amorphes recuites

The magnetic properties in the iron layers of Tb/Fe amorphous multilayers are investigated using ⁵⁷Fe Mössbauer spectrometry as a function of the nominal iron thickness and adequate heat treatment. We show that the perpendicular magnetic anisotropy is improved after homogenisation of the terbium-iron interface when the initial multilayer is of modulated composition Tb/Tb-Fe/Tb.